反应详情

温度

100 °C

To a round bottom flask was added (1-carbamoyl-cyclopropyl)-carbamic acid benzyl ester (935 mg, 4 mmol) in N,N-dimethylformamide dimethyl acetal (15 mL). The reaction mixture was stirred at 100° C. for 1 h. The solvent was concentrated in vacuo. The residue was dissolved in EtOAc/sat. NaHCO3. The organic phase was separated, washed with brine, dried over anhydrous Na2SO4, filtered, concentrated and dried under high vacuum to afford 1.11 g of (1-{[1-dimethylamino-meth-(E)-ylidene]-carbamoyl}-cyclopropyl)-carbamic acid benzyl ester as a light brown oil, m/z 290.9 [M+1]+.

1. concentrationThe solvent was concentrated in vacuo
2. dissolutionThe residue was dissolved in EtOAc/
3. customThe organic phase was separated
4. washwashed with brine
5. dry with materialdried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customdried under high vacuum